US5248660A - Process of preparing yttrium based superconductors - Google Patents

Process of preparing yttrium based superconductors Download PDF

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Publication number
US5248660A
US5248660A US07/814,874 US81487491A US5248660A US 5248660 A US5248660 A US 5248660A US 81487491 A US81487491 A US 81487491A US 5248660 A US5248660 A US 5248660A
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bacuo
plate
yba
rate
cuo
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US07/814,874
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Een H. Lee
I. Hun Song
Seok Y. Yoon
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Samsung Electro Mechanics Co Ltd
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Samsung Electro Mechanics Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/45—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on copper oxide or solid solutions thereof with other oxides
    • C04B35/4504—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on copper oxide or solid solutions thereof with other oxides containing rare earth oxides
    • C04B35/4508—Type 1-2-3
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/653—Processes involving a melting step
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00—Superconducting devices
    • H10N60/01—Manufacture or treatment
    • H10N60/0268—Manufacture or treatment of devices comprising copper oxide
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00—Superconducting devices
    • H10N60/01—Manufacture or treatment
    • H10N60/0268—Manufacture or treatment of devices comprising copper oxide
    • H10N60/0828—Introducing flux pinning centres
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S505/00—Superconductor technology: apparatus, material, process
    • Y10S505/725—Process of making or treating high tc, above 30 k, superconducting shaped material, article, or device
    • Y10S505/733—Rapid solidification, e.g. quenching, gas-atomizing, melt-spinning, roller-quenching
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S505/00—Superconductor technology: apparatus, material, process
    • Y10S505/725—Process of making or treating high tc, above 30 k, superconducting shaped material, article, or device
    • Y10S505/742—Annealing

Definitions

  • the present invention relates to a process of preparing yttrium-based superconductors, particularly to a process of preparing yttrium-based superconductors from a Y 2 BaCuO 5 compound reacting with liquid phase from a partially-melted YBa 2 Cu 3 O y compound.
  • melt processes wherein a fused superconducting compound is solidified slowly, have been studied and attempted successfully.
  • One of them is a quench and melt growth process (referred hereinafter as "QMG"), in which the stoichiometric compound of yttrium-based superconductors is heated rapidly to about 1400° C. to form a homogeneous melt, and then cooled slowly to produce a superconductor.
  • QMG quench and melt growth process
  • Partial melting is another melt process, in which a sintered stoichiometric superconductor is partially-melted to form a Y 2 BaCuO 5 phase and a liquid phase, and then is cooled slowly.
  • the YBa 2 Cu 3 O y superconductor is produced by the peritectic reaction of the Y 2 BaCuO 5 phase with the liquid phase.
  • the superconductors produced by these melt processes have large well-oriented grains with few voids, so that the weak-links are reduced drastically.
  • An objective of the present invention is to provide a process of preparing yttrium-based superconductors with reduced weak-links and having critical current densities greater than 10 4 A/cm 2 .
  • a Y 2 BaCuO 5 plate is made to react peritectically with the liquid phase from the partial-melted YBa 2 Cu 3 O y compound on it.
  • FIG. 1 illustrates a schematic configuration of a vertically stack assembly including (from the top), a body of YBa 2 Cu 3 O y compound, a Y 2 BaCuO 5 plate and a ZrO 2 plate used in the present invention.
  • FIG. 2(a) illustrates a heat-treatment schedule used in practicing the present invention.
  • FIG. 2(b) illustrates an enlargement of part A in FIG. 2(a).
  • FIG. 3 is a graph of magnetic field vs. magnetization for the superconductors manufactured in practicing the process of the present invention and in practicing the convention QMG method.
  • FIG. 4(a) is a SEM measurement of a superconductor prepared by the conventional QMG method.
  • FIG. 4(b) is a SEM measurement of superconductors prepared using the process of the present invention.
  • the present invention comprises the peritectic reaction of the Y 2 BaCuO 5 of a plate thereof with liquid phase BaCuO 2 .CuO, flowing down from a body of partially-melted YBa 2 Cu 3 O y which is supported on the body of Y 2 BaCuO 5 (FIG. 1).
  • the liquid phase forms during the partial-melting of the upper body of YBa 2 Cu 3 O y compound, and flows into the lower Y 2 BaCuO 5 plate.
  • the Y 2 BaCuO 5 plate reacts peritectically with the liquid BaCuO 2 .CuO to produce YBa 2 Cu 3 O y which grows in a preferred direction. Since the reaction occurs uniformly and homogeneously in the whole Y 2 BaCuO 5 plate, the resulting YBa 2 Cu 3 O y has large grains, with few voids, so that weak-links are reduced drastically. Thus the current density is greatly enhanced, usually to greater than 10 4 A/cm 2 .
  • the process of the present invention may comprise three steps: (1) partial-melting of YBa 2 Cu 3 O y compound located on the Y 2 BaCuO 5 plate to produce liquid phase BaCuO 2 .CuO, which flows down into the Y 2 BaCuO 5 plate, (2) peritectic reaction of the Y 2 BaCuO 5 of the upper plate, with the liquid phase BaCuO 2 .CuO, to form a YBa 2 Cu 3 O y phase, and (3) cooling and annealing the resulting body of YBa 2 Cu 3 O y to provide that body with superconducting properties.
  • step (1) it is recommended to heat the system to about 1100° C. at a rate of about 300° C./h and to hold it at that temperature for not less than 10 minutes. It is also recommended to quench the system to 1010° C. as rapidly as possible.
  • step (2) the peritectic reaction is made to occur while the system is cooled to 940° C. slowly at a rate of 2° C./h and held for about 10 hours at 940° C.
  • step (3) the system is cooled from 940° C. to 890° C. at a rate of 10° C./h, from 890° C. to 600° C. at a rate of 100° C./h, from 600° C. to 400° C.
  • the stoichiometric mixture of Y 2 O 3 , BaCO 3 , and CuO for YBa 2 Cu 3 O y was calcined twice at 920° C. for 24 hours, and sintered as a pellet at 950° C. for 24 hours in an oxygen atmosphere.
  • the mixture of Y 2 O 3 , BaCO 3 , and CuO for Y 2 BaCuO 5 stoichiometry was formed as a pellet and calcined in air at 950° C. for 24 hours.
  • the YBa 2 Cu 3 O y and Y 2 BaCuO 5 pellets which are respectively designated 123 and 211 in FIG. 1 were stacked on a ZrO 2 plates, as shown in FIG. 1.
  • This system was heat-treated following the schedule shown in FIG. 2. It was heated to 1100° C. at a rate of about 300° C./h and held for 10 minutes to partially-melt the upper body of YBa 2 Cu 3 O y compound. During this period, the liquid phase of BaCuO 2 .CuO flowed down into the lower Y 2 BaCuO 5 plate. After being quenched to 1010° C., the system was cooled to 940° C.
  • FIG. 3 The magnetization property (FIG. 3) was measured and compared with that of the superconductors manufactured by the prior QMG method.
  • FIG. 3 the magnetization curve of superconductors manufactured by the prior QMG method and by the present invention are represented by "•" and " ⁇ ", respectively. The estimation from this figure shows that the critical current density of the superconductor manufactured in the present invention was 2 times greater than that of the superconductors made by the prior QMG method.
  • the photos in FIG. 4 show the SEN measurements of the superconductors prepared by the conventional QMG method (a) and by this invention (b). Both superconductors have well-oriented grains with few voids.
  • the Y 2 BaCuO 5 phases in the present method are uniformly dispersed with a diameter of less than 1 ⁇ m. These fine Y 2 BaCuO 5 phases act as flux-pinning centers so that the critical current density is greatly enhanced.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
US07/814,874 1991-08-31 1991-12-31 Process of preparing yttrium based superconductors Expired - Lifetime US5248660A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR91-15194 1991-08-31
KR1019910015194A KR100209580B1 (ko) 1991-08-31 1991-08-31 이트륨계 초전도체의 제조방법

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
USH1399H (en) * 1993-07-06 1995-01-03 The United States Of America As Represented By The Secretary Of The Air Force Process for transforming pure Y2 BaCuO5 into a superconducting matrix of YBa2 Cu3 O7-x with fine and homogeneously dispersed Y2 BaCuO5 inclusions
US5496799A (en) * 1992-08-25 1996-03-05 Ngk Insulators, Ltd. Method for making rare earth superconductive composite
US5523284A (en) * 1992-11-05 1996-06-04 Alfred University Process for preparing a bulk textured superconductive material
US5525585A (en) * 1992-11-14 1996-06-11 Korea Advanced Institute Of Science And Technology Process for preparing YBa2 Cu3 O7-x superconductors
US5736489A (en) * 1997-02-07 1998-04-07 Wright State University Method of producing melt-processed polycrystalline YBa2 Cu3 O.sub.
US6083886A (en) * 1997-07-04 2000-07-04 Sumitomo Electric Industries, Ltd. Method of preparing oxide superconducting bulk body
US6830776B1 (en) * 2002-02-08 2004-12-14 The United States Of America As Represented By The Secretary Of The Air Force Method of manufacturing a high temperature superconductor
US20110260367A1 (en) * 2008-12-25 2011-10-27 Genesis Research Institute, Incorporated Transparent polycrystalline material and production process for the same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0319807A1 (en) * 1987-11-26 1989-06-14 Sumitomo Electric Industries Limited Method of manufacturing oxide superconductor
US4956336A (en) * 1989-02-10 1990-09-11 University Of Houston - University Park Oriented grained Y-Ba-Cu-O superconductors having high critical currents and method for producing same

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02103810A (ja) * 1988-10-11 1990-04-16 Tokai Univ 積層超電導皮膜
JPH0333051A (ja) * 1989-06-28 1991-02-13 Nippon Steel Corp 酸化物超電導バルク材料の製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0319807A1 (en) * 1987-11-26 1989-06-14 Sumitomo Electric Industries Limited Method of manufacturing oxide superconductor
US4994437A (en) * 1987-11-26 1991-02-19 Sumitomo Electric Industries, Ltd. Method of manufacturing oxide superconducting films by peritectic reaction
US4956336A (en) * 1989-02-10 1990-09-11 University Of Houston - University Park Oriented grained Y-Ba-Cu-O superconductors having high critical currents and method for producing same

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5496799A (en) * 1992-08-25 1996-03-05 Ngk Insulators, Ltd. Method for making rare earth superconductive composite
US5523284A (en) * 1992-11-05 1996-06-04 Alfred University Process for preparing a bulk textured superconductive material
US5525585A (en) * 1992-11-14 1996-06-11 Korea Advanced Institute Of Science And Technology Process for preparing YBa2 Cu3 O7-x superconductors
USH1399H (en) * 1993-07-06 1995-01-03 The United States Of America As Represented By The Secretary Of The Air Force Process for transforming pure Y2 BaCuO5 into a superconducting matrix of YBa2 Cu3 O7-x with fine and homogeneously dispersed Y2 BaCuO5 inclusions
US5736489A (en) * 1997-02-07 1998-04-07 Wright State University Method of producing melt-processed polycrystalline YBa2 Cu3 O.sub.
US6083886A (en) * 1997-07-04 2000-07-04 Sumitomo Electric Industries, Ltd. Method of preparing oxide superconducting bulk body
US6830776B1 (en) * 2002-02-08 2004-12-14 The United States Of America As Represented By The Secretary Of The Air Force Method of manufacturing a high temperature superconductor
US20110260367A1 (en) * 2008-12-25 2011-10-27 Genesis Research Institute, Incorporated Transparent polycrystalline material and production process for the same
US8470724B2 (en) * 2008-12-25 2013-06-25 Inter-University Research Institute Corporation, National Institutes Of Natural Sciences Transparent polycrystalline material and production process for the same

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JP2672926B2 (ja) 1997-11-05
KR930004487A (ko) 1993-03-22
KR100209580B1 (ko) 1999-07-15
JPH05201729A (ja) 1993-08-10

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